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Dental Research
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Influence of Test Method on Failure Stress of Brittle Dental Materials


S. Ban and K.J. Anusavice
J DENT RES 1990 69: 1791
DOI: 10.1177/00220345900690120201
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Influence of Test Method on Failure Stress of Brittle Dental Materials


S. BAN and K.J. ANUSAVICE'
Department of Dental Materials Science, School of Dentistry, Aichi-Gakuin University, Chikusa-ku, Nagoya 464, Japan; and 'Department of
Dental Biomaterials, College of Dentistry, University of Florida, Gainesville, Florida 32610-0446

A bi-axial flexure test (piston-on-three-balls), a four-point flexure test, and a diametral tensile test were used to measure the
failure stress of four brittle dental materials: zinc phosphate
cement, body porcelain, opaque porcelain, and visible lightcured resin composite. Furthermore, the fracture probability
of the bi-axial test specimens was predicted from the results
of the four-point flexure test, with use of statistical fracture
theory. Bi-axial failure stresses calculated from an equation
developed by Marshall (1980) exhibited no significant difference for zinc phosphate cement as a function of piston size,
specimen thickness, presence or absence of a stress-distributing film, and loading rate. The four-point flexure strength values of zinc phosphate cement and opaque porcelain were
significantly lower (p<0.05) than the corresponding mean biaxial strength values, while the mean four-point flexure strength
values of body porcelain and resin composite were not significantly lower (p>0.05) than the corresponding mean bi-axial
strength values. The diametral tensile strength of all materials
was significantly lower than the bi-axial flexure strength. The
mean bi-axial flexure strengths of zinc phosphate cement and
opaque porcelain were much higher than the theoretical values
predicted from surface flaw theory, while the strength values
for body porcelain and resin composite were comparable with
those determined from the four-point flexure test. These results
demonstrate that the strength of zinc phosphate cement depends not only upon the geometric factors, but also upon sample preparation conditions.
J Dent Res 69(12):1791-1799, December, 1990

Introduction.
Mechanical strength is an important factor that controls the
clinical success of dental restorations. Usually, complex stress
distributions that are induced by compressive, tensile, and shear
stresses are present in most specimens under practical conditions. It is extremely difficult to induce a pure stress of a single
type in a body. In general, tensile strength is easily determined
for ductile materials such as metals. For convenience, compressive strength is often measured for brittle materials such
as porcelains, cements, amalgams, and resin composites.
However, brittle materials are much weaker in tension than in
compression, and tensile stresses in some materials are (in
certain cases) larger than compressive stress (Anusavice and
Hojjatie, 1987). Therefore, tensile strength is generally considered as the more meaningful property for these brittle materials (compared with compressive strength) for assessment
of the failure potential of dental restorations, especially in the
presence of critical surface flaws.
To determine the tensile strength for brittle dental materials,
the diametral tensile test has been used frequently (Earnshaw
and Smith, 1966; Williams and Smith, 1971; Powers et al.,
Received for publication February 27, 1990
Accepted for publication August 2, 1990
This study was supported by NIDR Grant DE 06672.

1976). The traditional tensile test has rarely been used for
brittle materials (Bowen and Rodriguez, 1962; Zidan et al.,
1980) because of the difficulty associated with gripping and
aligning the specimens. The diametral tensile test provides a
simple experimental method for measurement of the tensile
strength of brittle materials. However, the complex stress distribution developed in the specimen can lead to various modes
of fracture. If the specimen deforms significantly before failure, the data may not be valid. Zidan et al. (1980) suggested
that the diametral tensile test cannot be considered reliable for
dental resinous materials. Chiang and Tesk (1989) demonstrated that a correction of the stress calculation equation for
diametral tension is needed with double cleft fracture.
The main advantage of the flexure test is that a state of pure
tension can be established on one side of the specimen (Berenbaum and Brodie, 1959). Three-point and four-point flexure
tests have also been used for strength evaluation of singlecomponent brittle materials (Bryant and Mahler, 1986; Soderholm, 1986) and metal-ceramic structures (Coffey et al.,
1988). For these uni-axial flexure tests, the principal stress on
the lower surfaces of the specimens is tensile, and it is usually
responsible for crack initiation in brittle materials. However,
undesirable edge fracture (which can increase the variance of
the failure stress value) can occur. Furthermore, these methods
were designed for engineering materials that are usually associated with relatively large specimens. For brittle dental materials, construction of such specimens is not usually convenient
because suitable quantities of dental restorative materials are
not often available to prepare a sufficient number of specimens
for assessment of statistically significant differences. Furthermore, the residual stress states due to polymerization shrinkage
or thermal contraction difference and the flaw characteristics
induced in large specimens may not be representative of those
that are present in smaller clinical restorations.
Recently, the bi-axial flexure test has been used frequently
for the determination of fracture characteristics of brittle materials. The measurement of the strength of brittle materials
under bi-axial flexure conditions rather than uni-axial flexure
is often considered more reliable, because the maximum tensile
stresses occur within the central loading area and spurious edge
failures are eliminated. This allows slightly warped specimens
to be tested and produces results unaffected by the edge condition of the specimen. This feature makes the method suitable
for assessment of the effects of surface conditions on strength.
A wide variety of loading arrangements has been developed
for bi-axial flexure tests: (1) ring-on-ring (Kao et al., 1971),
(2) piston-on-ring (Wilshaw, 1968), (3) ball-on-ring (McKinney and Herbert, 1970), (4) ring-on-ball (Shetty et al.,
1983), (5) piston-on-three-ball (Kirstein and Woolley, 1967),
and (6) ring-on-spring (Marshall, 1980). For this study, the
fifth option was used, since it is suitable for slightly warped
and small specimens such as brittle dental materials, and excellent results by this method have been reported previously
for some glasses and ceramics. The bi-axial flexure strength
is determined by support of a disc specimen on three metal
spheres positioned at equal distances from each other and from
the center of the disc. The load is applied to the center of the
1791

1792

BAN & ANUSA VICE

Code

Type

ZP
BP

Zinc Phosphate Cement

OP
RC

Body Porcelain
Opaque Porcelain
Resin Composite

J Dent Res December 1990


TABLE 1
MATERIALS TESTED
Brand Name
Orthodontic Cement with Fluoride
White Body #2
White Opaque #4
Herculite XR

Manufacturer

Ormco, Glendora, CA
J.F. Jelenko & Co., Armonk, NY
J.F. Jelenko & Co.
Kerr Manufacturing Co., Romulus, MI

TABLE 2

SPECIMEN DIMENSIONS (mm)


Four-point Flexure Test
1
w

ZP
BP
OP
RC
D,

Bi-axial Flexure Test


D
t
0.8 0.1
12.7 0.1
S
M
13.6 0.1
1.3 0.1
33.7 + 0.5
6.8 0.1
L
2.6 + 0.2
15.8 0.1
14.4 1.0
1.9 0.3
4.9 0.2
28.9 0.3
14.4 + 0.1
2.0 - 0.1
29.8 + 0.2
5.0 0.4
1.2 + 0.1
3.1 + 0.1
13.7 0.2
36.0 0.2
diameter of specimen; t, thickness of specimen; 1, length of specimen; w, width of specimen; S,

opposite surface by a flat piston. Kirstein and Woolley (1967)


demonstrated that stresses in a thin, circular aluminum-alloy
plate were independent of angular orientation and the number
of supports.
Wachtman et al. (1972) reported that bi-axial flexure strength
values for eight types of alumina show that a coefficient of
variation of about 7% can be achieved by testing five specimens and that different laboratories generally obtain good
agreement on strength values. Marshall (1980) modified the
stress equation to correct for geometry effects and demonstrated that the stress calculated from this modified equation
for two types of glasses was in good agreement with the stress
measured from strain gauges. Pletka and Wiederhorn (1982)
compared the failure characteristics of specimens fractured in
bi-axial flexure tests with those fractured by means of a conventional four-point flexure test. Morena et al. (1986) investigated the dynamic fatigue of dental porcelain using a bi-axial
flexure test. Usually, disc specimens (12-50 mm in diameter
and 1-3 mm in thickness) are used for these tests. They can
be easily made under typical restorative conditions. Furthermore, the flat surface of the test specimen can be easily controlled by conventional metallographic polishing methods and
typical dental finishing techniques.
The objectives of this study were: (1) to test the hypothesis
that the bi-axial flexure test reduces the variance of fracture
strength values for brittle dental materials with various levels
of homogeneity, compared with the four-point flexure test and
the diametral tensile test, and (2) to analyze the influence of
specimen geometry on the mean fracture strength values for
brittle dental materials by use of fracture statistics.

Materials and methods.


Specimen preparation. -For bi-axial flexure measurements,
disc specimens were prepared for an orthodontic zinc phosphate cement, a feldspathic body porcelain, a feldspathic opaque
porcelain, and a visible-light-cured resin composite (Table 1).
Zinc phosphate cement specimens were prepared by conventional techniques according to the solubility test of ADA Specification No. 8 for zinc phosphate cement. The powder/liquid
ratio was 3/1 (1.5 g/0.5 mL). Approximately 0.5 mL of cement
of standard consistency was placed on a flat glass plate. Three
ring sizes (inner diameter/thickness ratios of 13/0.6, 14/1.2,
and 16/2.4 mm) were placed in the soft cement, and another
glass plate was used to press the cement into a disk. Three

t
6.7 0.2

Diametral Tensile Test


t
D
6.2 0.1

4.3 0.2
7.7 0.1
4.3 0.4
7.8 0.1
3.1 + 0.1
6.2 + 0.0
small; M, medium; and L, large.

3.2 0.1

3.5 + 0.5
3.3 0.3
3.2 0.1

minutes after the mix was started, the glass plates and cements
were placed in a humidor at 37C for one h. After removal
from the humidor, the specimens were separated from the glass
and stored in water at 37C for 24 h.
Porcelain specimens were prepared by normal fabrication
procedures. A slurry of porcelain powder was vibrated and
condensed into a mold 16 mm in diameter and 2 mm in depth.
The discs were fired in a dental oven (Mark IV, J.M. Ney
Co., Bloomfield, CT) at a heating rate of 55C/min under
vacuum to 982C followed by a 90-second holding time in air.
The specimens were removed from the furnace and rapidly
cooled in ambient air by natural convection. The porcelain
discs were ground from 120-grit to 600-grit papers and polished with 1->Lm and 0.3-gm A1203 powder on a metallographic polishing wheel.
Visible-light-cured resin composite specimens were made as
follows: Approximately 0.5 mL of resin paste was placed on
a flat glass plate, 1.0 mm in thickness. A flexible ring, approximately 14 mm in inner diameter and 1.2 mm in thickness,
was placed in the paste, and another glass plate was used to
press the resin paste into a disc. Light emitted from a fiber
optic handpiece (Translux, Kulzer & Co., Bad Homburg, Germany) passed through the glass plates for a total of 200 s so
that adequate polymerization of each side would be ensured.
After light irradiation, specimens were separated from the glass
plates and stored in water at 37C for 24 h before being tested.
Specimens for the four-point flexure and the diametral tensile tests were also prepared in a similar manner. The final
dimensions of the specimens are listed in Table 2.
Determination of fracture strength. -The bi-axial flexure
test apparatus is described in the ASTM Standard F394 for biaxial flexure testing of ceramic substrates. In this study, the
dimensions of the apparatus were smaller than those described
in the ASTM standard so that the small specimen size of brittle
dental materials typically used in dental restorations would be
accommodated.
As shown in Fig. 1, specimens were supported on three steel
spheres (3.2 mm in diameter) equally spaced along a diameter
of 10 mm. For zinc phosphate cement specimens, loading was
applied by a steel piston (with flat areas of 1.2 mm and 1.6
mm in diameter ground along the surface of contact) until
fracture occurred. For the porcelain and resin composite specimens, the piston with a diameter of 1.2 mm was used.
The failure stress, cr, at the center of the lower surface was
calculated by equations developed by Marshall (1980). These

Vol. 69 No. 12

FAILURE STRESS OF BRITTLE DENTAL MATERIALS

equations were based on the bi-axial flexure test developed by


Wachtman et al. (1972), and original equations derived by
Kirstein and Woolley (1967). The failure stress, a, can be
expressed as:
A p / t2
(1)
and
A = (3/4r) [2 (1 +v) in (a/ro*)
+ (1-v) (2 a2-ro*2)/2 b2 + (1 + v)] (2)
where P is the applied load at failure, v is Poisson's ratio, a
is the radius of the support circle, b is the radius of disc specimen, ro* is the equivalent radius given in ro* = (1.6 r02 +
2))1/22-0.675t, t is the thickness of the disc specimen, and ro
is the radius of the piston at the surface of contact.
If a series of nearly identical specimens is tested, the factors
A and t (which depend only on the dimensions and Poisson's
ratio) are constant, so the equation reduces to a simple proportionality between load and stress. In this study, the strength
values were calculated with Poisson's ratio values of 0.35 for
cement, 0.28 for porcelain (Anusavice and Hojjatie, 1987),
and 0.24 for resin composite (Craig, 1989).
Tests were usually carried out in air at room temperature
using a thin plastic film (about 50 pum in thickness) between
the piston and the upper surface of the specimen, to assist in
obtaining uniform loading over the surfaces of the discs. Crosshead loading rates of 0.1 and 1 mm/min were applied by a
universal testing machine (Instron Universal Testing Machine
Model 1125, Instron Corp., Canton, MA). For investigation
of the effects of piston diameter, disc diameter, and loading
rate on the bi-axial fracture strength of a brittle dental material,
an orthodontic zinc phosphate cement was used.
For the four-point flexure test, the rectangular specimens
were supported by two 3-mm-diameter rods set 21 mm apart.
The load was applied by two rods that were set 7 mm apart.
A cross-head loading rate of 0.2 mm/min was used. The maximum tensile stress was calculated by the equation:
uJ = PL/wt2
(3)
where P is the applied load at failure, L is the length of outer
span, w is the width of the specimen, and t is the thickness of
the specimen.
For the diametral tensile test, cylindrical specimens were
tested at a cross-head loading rate of 0.1 mm/min. The maximum tensile stress for the diametral test is given by the equation:
-=2 P / rrDt
(4)
where P is the applied load at failure, D is the diameter of the
specimen, and t is the thickness of the specimen. From these
data, the mean value, standard deviation, and coefficient of
variation were calculated. Fracture surfaces representative of
each group of specimens were characterized by means of scanning electron microscopy (SEM: JSM-35C, JEOL Ltd., Tokyo, Japan).
Fracture statistics. -The failure strengths of brittle materials are statistically distributed as a function of the homogeneity of the material (Ritter, 1986). One commonly used
statistic for the description of this distribution is the Weibull
distribution, which is given by:
Pf = 1-exp [-(-/U)m]
(5)
where Pf is the fracture probability defined by the relation
Pf=i/(N+1), i is the rank in strength, N denotes the total
number of specimens in the sample, m is the shape parameter,

1 793

which is called the Weibull modulus, and u,,, is the scale


parameter or characteristic strength. Higher values of Weibull
modulus correspond to a higher level of homogeneity of the
material. Most ceramics are reported to have m values in the
range of 5 to 15, whereas metals, which fail in a ductile manner, have m values in the range of 30 to 100 (Johnson, 1983).
The Weibull modulus, characteristic strength, and strength at
a predicted failure level of 5% were obtained with use of a
computer program designed to carry out the Weibull analysis
from the fracture data.
This analytical method is very popular because of its ease
of application. However, the Weibull approach is not based
on physical principles, but is based on statistical concepts.
Therefore, as pointed out by several investigators (Giovan and
Sines, 1979; Shetty et al., 1983; Lamon and Evans, 1983),
the Weibull analysis has some limitations that challenge its
ability to predict failure of components having complex geometries and which are subjected to a multi-axial stress state. This
problem may be crucial for components used in dental restorations having complex geometries and subjected to multi-axial
stress states.
The elemental strength approach (Evans, 1982) represents a
more physical analysis of failure, based essentially on the premise

Load
Piston
2ro

jXTjj~~~ _Specimen
Support

Ball Bearing

Specimen
Holder

Fig. 1-Schematic illustration of piston-on-three-ball bi-axial flexure test.


a, the radius of the support circle; b, the radius of disc specimen; t, the
thickness of the specimen; and r, the radius of the piston at the surface
of contact.

1794

J Dent Res December 1990

BAN & ANUSA VICE

TABLE 3
BI-AXIAL FLEXURE TEST RESULTS FOR ZINC PHOSPHATE CEMENT
Condition
Specimen
Diameter
LoadLoading
Meant
of Piston
distributing
Speed
No. of
Strength
Size*
Film
Tests
Code
(mm)
(mm/min)
(MPa)
Yes
0.1
M
1.2
10
18.1
ZP
10
Yes
0.1
19.0
1.2
ZP1
S
16.9
Yes
0.1
10
L
1.2
ZP2
0.1
10
19.2
Yes
M
1.6
ZP3
17.3
1.2
No
0.1
10
ZP4
M
17.5
Yes
1.0
10
M
1.2
ZP5
60
18.0
Total
*Dimensions of S, M, and L specimens are indicated in Table 2.
tCommon vertical lines indicate no significant difference at ox = 0.05.

that a specimen body contains a distribution of cracks that can


be characterized by their flaw-extension stress. A multi-axial
elemental strength model was derived by Lamon and Evans
(1983) and applied to specific test geometries, providing an
experimental demonstration of practical requirements for a multiaxial analysis of fracture. However, these approaches are
mathematically complex and require extensive numerical analysis
even for simple stress states. Shetty et al. (1983) used the
Barnett-Freudenthal approximation (Batdorf, 1977) for comparison of bi-axial data with uni-axial data from three- and
four-point flexure tests.
In the present study, the failure probability of brittle specimens subjected to bi-axial flexure was calculated from the
results of the four-point flexure test, by use of the following
statistical fracture theory. Eq. (5) can be converted to the following equation:

Result
Standard

Coefficient

Deviation

of
Variation
0.073
0.098

(MPa)
1.3
1.9
2.6
2.1
2.5
2.0
2.2

0.155

0.108
0.142
0.113
0.121

Weibull introduced this transformation of scale parameters to


relate the multi-axial stress state to the uni-axial stress condition. Eq. (9) can be integrated in closed form giving:
(11)
Bs = (or a2) (oru/or)m Ls
where o,,L is the maximum stress at the center of the disc specimen and L. is the loading factor,

L,

(ot + P)/(m + 1)Oc

(12)

and
a

3P(3+v)a2/8

t2oal

(13)
(14)

P = 3 P (1 +3v) a2/8 t2oL


From Eqs. (6) and (11),
In In [1/(1 - Pf)] m[ln (oa) - Cj]
(15)
where
C= In (o,) - ln(ir a2 L,)/m
(16)
In a similar way, the risk of rupture in bi-axial tension, Bv,
for failure caused by a volume flaw can be given as follows:
B, = (ir a2t/2)(cr/cr0)n'Lv
(17)
(18)
Lv ((x + 3)/(m + 1)2 a
and
In In [1/(1 -Pf)] m[ln (a,,) CQ
(19)
where
C= In (or,) - ln (orr a2t/2 L,)/m
(20)
With these equations, statistics parameters for the bi-axial test
can be predicted from the four-point flexure test. The loading
factor is one convenient parameter for this purpose, because it
incorporates the stress-state and stress-gradient effects into the
fracture statistics. The loading factors decrease with increasing
Weibull modulus, reflecting the influence of stress gradients.
The volume loading factors are smaller than the surface loading
factors because of the additional stress gradient in the axial
direction. In the present study, the failure probability for the
bi-axial test of four brittle dental materials was predicted from
the Weibull parameters for the four-point flexure test by means
of these equations.
=

Pf

exp [-B]

(6)

where B is the risk of rupture. For multi-axial stress states, B


is defined at any point in a stressed body as
dB = f, n(orn)dw
(7)
where n(o-,) is a characteristic material function; o(n is the normal tensile stress at an arbitrary angle relative to the principal
stresses crl, 02, and O3; and dwo an elemental area on a unit
solid sphere. The geometric variables used to describe and
dw are defined in an orientation relative to principal stresses.
Eq. (7) is evaluated by integration of those portions of the unitsphere where orn is tensile. Weibull assumed that B was zero
for orientations for which oa, was compressive. For the uniaxial stress case, the two-parameter form is
n (cn)
(8)
(3nlcJno)
where m is a shape parameter, or Weibull modulus, and or,,
is a scale parameter, as described previously.
For the disc specimen subjected to uniform loading pressure,
bi-axial tension causes failure due to surface flaws. According
to the Barnett-Freudenthal approximation (Batdorf, 1977), the
principal stresses are assumed to act independently. This assumption leads to the following equation for the risk of rupture
in bi-axial tension, B5, due to surface flaw effects:
B
2rr fr(ulrcvo)m r dr + 2r fr (alao0)m r dr (9)
where or is the radial stress and or, is the tangential stress. For
the uniform-pressure-on-disc specimen, the stress state is biaxial tension, with a,= 0r, U2 =ot, and C3= 0. ao, is related
to cr,, through the equation
ao-" = [(2m + 1)/2 'j]u "(m(10)
o,,

Results.
The mean bi-axial flexure strength values of zinc phosphate
cement as a function of six different test conditions are listed

FAILURE STRESS OF BRITTLE DENTAL MATERIALS

Vol. 69 No. 12

1 795

TABLE 4

COMPARATIVE DATA FOR THE THREE TEST METHODS

Specimen
Bi-axial flexure test
ZP*
BP
OP
RC
Four-point flexure test
ZP
BP
OP
RC
Diametral tensile test
ZP
BP
OP
RC
*Same data as in Table 3

Ratio of
Strength to
Bi-axial Flex-

No. of
Tests

Meant
Strength
(MPa)

Standard
Deviation
(MPa)

Coefficient
of
Variation

10
10
10
10

18.1
52.4
75.6
103.9

1.3
5.6
8.6
15.6

0.073
0.106
0.114
0.150

1
1
1
1

10
10
10
10

6.8
48.4
52.4
98.4

0.6
5.8
10.2
11.4

0.088
0.125
0.195
0.116

0.375
0.923
0.693
0.947

4.5
22.4
23.8
24.6

0.5
8.7
6.0
5.8

0.088
0.391
0.253
0.234

0.249
0.427
0.315
0.236

10
10
10
10
for group ZP.

ure
Strength

tCommon vertical lines indicate no significant statistical difference at a = 0.05.

in Table 3. The mean strength for these conditions was not


significantly different at the 95% confidence level when Duncan's multiple range test was used. Although zinc phosphate
cement was mixed manually for each specimen, the coefficient
of variation fell within a narrow acceptable range (0.073 to
0.155), indicating the adequacy of the experimental data for
evaluation of the strength of the cement. The bi-axial flexure
strength of zinc phosphate cement was insensitive to specimen
size, diameter of the piston, use of a load-distributing film,
and loading speed. Fractured specimens could be grouped according to a two-segment or three-segment fracture pattern.
However, no relationship between the fracture mode and the
strength was observed. Based on these results, the test conditions for specimen group ZP (Table 3) used for zinc phosphate cement were used as the standard test conditions for
subsequent bi-axial testing, since the results under these conditions showed the smallest coefficient of variation, and since
the mean bi-axial strength represented the mean of the six
groups tested.
The fracture strength of the brittle dental materials measured
by the three different test methods is summarized in Table 4.
For the bi-axial flexure test, resin composite exhibited the largest mean bi-axial strength. The mean bi-axial flexure strength
of opaque porcelain was significantly higher (p<0.05) than
that of body porcelain.
The mean strength based on four-point flexure of zinc phosphate cement and opaque porcelain was significantly lower
(p <0.05) than their corresponding bi-axial strength values. Zinc
phosphate cement exhibited the smallest ratio (0.375) of fourpoint to bi-axial flexure strength, while opaque porcelain exhibited a ratio of 0.693. The mean four-point flexure strengths
of both porcelains were not significantly different (p<0.05).
The four-point flexure strength values of body porcelain and
resin composite were not significantly different (p > 0.05) from
their corresponding bi-axial flexure strengths. There were no
significant differences (p>0.05) between the coefficient of
variation of bi-axial and four-point flexure strength for these
four materials.
The diametral tensile strength of the four materials was much
lower than the corresponding bi-axial flexure strength. The
ratio of diametral to bi-axial strength ranged from 0.236 to

0.427 for the four materials. There were no significant differences (p>0.05) among the diametral tensile strengths of body
porcelain, opaque porcelain, and resin composite. The diametral tensile test data revealed that zinc phosphate cement
exhibited the lowest coefficient of variation of 0.088, while
other materials exhibited relatively larger values of 0.234 to
0.391.
Shown in Fig. 2 are Weibull plots of fracture stresses, In In
[1/(1 -Ff)] vs. ln u, for the zinc phosphate cement tested according to the three methods. The data points were described
by a straight line produced by least-squares fit of the fracture
data by use of a computer, and the Weibull modulus, characteristic strength, and strength at a predicted failure level of
5% were also calculated by computer. These results are listed
in Table 5. The Weibull moduli for both bi-axial and fourpoint flexure tests were larger than those for the diametral
tensile test, except for zinc phosphate cement. The Weibull
modulus of zinc phosphate cement exhibited the largest value
for each test method.
Shown in Table 6 are the failure probability parameters for
the bi-axial flexure test of four brittle dental materials derived
from the analytical solutions of Eqs. (11) to (20) by use of
Weibull analysis results for the four-point flexure test in Table
5. Predicted plots (Bs and B,) for the Weibull analysis of the
zinc phosphate cement are presented as dashed lines in Fig. 2.
Experimental results for the bi-axial test of zinc phosphate
cement and opaque porcelain showed much higher strength
than that predicted by surface flaw analysis. The failure probability of both body porcelain and resin composite exhibited
good agreement with the values predicted for the surface flaw

condition.
Shown in Fig. 3 are SEM images of fracture surfaces produced by bi-axial and four-point flexure stress for zinc phosphate cement, body porcelain, opaque porcelain, and resin
composite. The arrows indicate the most likely sites of crack
initiation. The fracture surfaces for zinc phosphate cement
specimens exhibited a porous structure, especially in the specimens that were prepared for the four-point flexure test, which
had much larger pores than those for the bi-axial test. For the
specimens tested by four-point flexure, the fracture origin appeared to be located around pores located at the corner of the

1796

J Dent Res December 1990

BAN & ANUSA VICE

TABLE 5
SUMMARY OF WEIBULL ANALYSIS

2
ZP

Specimen
Bi-axial flexure test
ZP
BP
OP
RC
Four-point flexure test
ZP
BP

Cc

o.a05

(MPa)

(MPa)

10.45
7.54
7.47
6.27

18.6
54.9
80.2
111.6

14.0
37.0
53.9
69.5

Diametral

Four-point

Biaxial

A
CL
-

8.95
8.85
4.37
6.88

7.1
50.6
57.1
102.9

5.1
36.2
29.0
66.8

ZP
11.68
BP
2.10
3.25
OP
RC
3.39
m, Weibull modulus.
or, characteristic strength.

4.7

3.7
6.9
10.5
11.0

OP
RC
Diametral tensile test

1-

-1

-2

25.9
26.2
26.3

cT0.05, strength predicted at the 5% level of failure.


fracture surface. The fracture surface of opaque porcelain produced by four-point flexure also showed large pores, which
were associated with the crack origin, while that for the biaxial flexure test showed a homogeneous structure having small
pores. The fracture surfaces of body porcelain and resin composite for both flexure tests exhibited a similar structure that
could be characterized as homogeneous and low in porosity.

Discussion.
Effects of test conditions on bi-axialflexure strength. -Maximum tensile stresses produced by bi-axial flexure occur below
the central loading area on the bottom surfaces of disc specimens. However, because of the typically high elastic modulus
and hardness of brittle materials, any imperfect contact between the rigid loading tool and the test specimen can lead to
a substantial deviation from radial symmetry in the stress field
and, consequently, to errors in strength measurements. Wachtman et al. (1972) suggested that a layer of polyethylene between piston and test surface would assist in the obtaining of
uniform loading at the end of the piston. Based on strain gauge
measurements, Marshall (1980) found that the piston applies
the load uniformly over its contact area when a film is used.
However, in the present study, there were no significant differences (p>0.05) between the strengths of zinc phosphate
cement with and without a film. It seems that the specimen
surface of zinc phosphate cement, which is covered with a
precipitate by reaction between the cement surface and water
in the storage chamber, was flattened by the initial contact of
the piston and, consequently, developed a uniform loading
condition without an intermediate film. Furthermore, if the flat
surface of the piston is sufficiently parallel to the test surface,
one does not always need to place the film or cushion over the
specimen center.
The thickness of the specimens is one of the most important
factors in the determination of the bi-axial flexure strength,
since the calculated stress is inversely proportional to the second power of its thickness, as derived in Eq. (1). Furthermore,
the stress equation is valid only if the deflection does not exceed about one-half of the plate thickness (Wachtman et al.,
1972). Bending is directly proportional to the sustained load
and inversely proportional to Young's modulus, whereas it is
only slightly dependent on Poisson's ratio. The estimated min-

-3 - _
0.5

B;
1.0

1.5

Bv
2.0

In

2.5

3.0

3.5

(MPa)

Fig. 2-Weibull plots of bi-axial flexure strength, four-point flexure


strength, and diametral tensile strength for zinc phosphate cement (ZP).
Solid lines represent regression analyses of the raw data for the three test
methods, and dashed lines represent predictions (Bs, Bv) of bi-axial flexure
strength from four-point-flexure-strength data.

imum specimen thickness was calculated according to ASTM


Standard F394. Within the stress range (18-180 MPa) encountered in this study and over a Young's modulus range for brittle
materials [13.7 GPa for zinc phosphate cement, 16.6 GPa for
resin composite, and 69 GPa for porcelain (Craig, 1989)], the
estimated minimum thickness was always less than that encountered in the test. Therefore, it is reasonable to assume that
the use of this stress equation was valid in the present study.
Dimensions of the piston and specimen are included as factors in the stress Eq. (1) for the bi-axial flexure test. The
important assumption of this equation is that the specimen
structure was homogeneous. However, brittle dental materials
used in the present study were not considered as homogeneous
materials. For example, zinc phosphate cement contains significant porosity, matrix, and unreacted cement powders, as
shown in Fig. 3. However, as shown in Table 3, the bi-axial
strengths of the specimens with different dimensions were not
significantly different (p>0.05). Although the effects of geometry have been identified in various strength tests (Baratta,
1984; Ikeda et al., 1986; Lamon, 1988), it is concluded that
the effect of geometry on bi-axial strength is negligible. Perhaps a more important factor in future refinement of these tests
is the design of more uniform load distribution at load application and load-supporting regions to minimize the risk of localized failure at these locations. Some of the variance of
measured strength values can be explained on the basis of a
few two-segment fractures vs. the more common three-segment fractures. The two-segment fractures may indicate that
some of these were initiated at the load-application or loadsupport regions.
The strengths of brittle materials generally increase with
increasing loading rate. The dependence of strength stressing rate, caused by subcritical crack growth, has been described by Evans (1974) as follows:
on

orf

where af is fracture stress at

stress rate, C is constant, and

C 6rl/(l + n)
a
n

(21)

given stressing rate, a is the


is a crack-propagation param-

Vol. 69 No. 12

FAILURE STRESS OF BRITTLE DENTAL MATERIALS

1797

TABLE 6

PREDICTED FAILURE PROBABILITY PARAMETERS FOR BI-AXIAL FLEXURE STRENGTH BASED ON FOUR-POINT FLEXURE DATA
Surface Flaw
Volume Flaw
In ('rr a2L9)/m
L
ln [(QT a2tl2)L,]/m
ln oC
Code
L,
cv
- 0.288
0.002
2.371
0.015
0.020
2.063
ZP
2.083
4.274
0.002
- 0.258
0.045
3.971
BP
4.016
0.017
0.161
0.026
3.984
0.005
-0.221
4.366
OP
4.145
5.062
0.020
4.691
0.003
- 0.304
0.067
RC
4.758

eter. These n values vary appreciably from one material to


another (Pletka and Wiederhorn, 1978; Morena et al., 1986).
In the present study, there was no significant difference (p > 0.05)
between the results determined at a loading rate of 0.1 mm/
min and 1 mm/min, which correspond to stressing rates of
0.64 and 6.4 MPa/s, respectively. These two loading rates are
often used for mechanical testing. It seems that zinc phosphate
cement has a small value of n, which implies that it is susceptible to fast crack propagation.
The strength values for these different test conditions showed
good agreement with the calculated stress values when Eq. (1)
was used. Thus, it is concluded that the bi-axial flexure test
represents a reliable method for determinations of the strength
of brittle dental materials, since it is relatively insensitive to
test conditions. However, it should be noted that the four-point
flexure specimens were fairly large in this study, and some of
these results may have reflected variations caused by incon-

sistencies in mixing.
Comparison with four-point flexure strength.-Shetty et al.

(1983) reported that the bi-axial flexure strength of alumina


was higher than its four-point flexure strength and lower than
its three-point flexure strength, and they compared bi-axial
strength with predictions based on four-point flexure data. They
found that Weibull statistics provided a good description of
the size effects on data from the two uni-axial tests, but underestimated the effect of stress bi-axiality. On the other hand,
Pletka and Wiederhorn (1978) reported that the four-point flexure strength of magnesium aluminosilicate glass in water was
higher than its bi-axial flexure strength in water. Giovan and
Sines (1979) showed that the bi-axial flexure strength of dense
alumina was 8.5 and 8.1% lower than the uni-axial strength
for ground and lapped surfaces, respectively. Pletka and Wiederhorn (1982) showed a consistent relationship between biaxial and four-point flexure strength data for five types of
ceramics over a range of stressing rates. In contrast, the present
study showed that there was no consistent relationship between
uni-axial and bi-axial flexure strength data.
The first reason for this inconsistency is the surface condition of the specimens. The surfaces of the specimens contain
many artificial flaws, since they were ground through 600-grit
(Shetty et al., 1983), 400-mesh (Pletka and Wiederhorn, 1978),
and 320-grit (Giovan and Sines, 1979) diamond abrasives. The
specimens in the present study were polished through 0.3-pLm
alumina powder for each porcelain, and zinc phosphate cement
and resin composite specimens were flattened by glass plates

during setting.
The second reason for the discrepancy is the specimen size
effect. The effect of specimen size on four-point flexure strength
has been reported by many investigators (Berenbaum and Brodie, 1959; Baratta, 1984; Ikeda et al., 1986; Lamon, 1988).
Berenbaum and Brodie (1959) showed that the four-point flexure strength of pure plaster of Paris increased with a decrease
in specimen thickness. They suggested that the four-point flexure strength of porous, weak, and brittle materials such as
plaster is strongly influenced by specimen size. The surface
layer of these chemically setting materials is tougher than their

internal structure, since the surface tends to form a dense structure having few pores during setting under pressure with the
mold, as shown in Fig. 3. Furthermore, the properties of mixing materials such as plaster and cement are significantly affected by the total volume of mixing. For preparation of zinc
phosphate cement specimens for the four-point flexure test, the
mixture of 6 g of powder and 2 mL of liquid was used, while
a standard amount of powder and liquid (1.5 g and 0.5 mL)
was used for preparation of specimens for the bi-axial flexure
test. Larger pores were formed and remained in the specimens
for the four-point flexure test, compared with the bi-axial flexure test specimens, because of insufficient mixing and pressure. Thus, the bi-axial testing of zinc phosphate cement yielded
much higher strength values than those predicted for both surface-flaw failure and volume-flaw failure, possibly because of
differences in the homogeneity of specimens. Opaque porcelain specimens were also relatively inhomogeneous. Compared
with body porcelain, opaque porcelain is relatively difficult to
condense for large specimen volumes such as that used for the
four-point flexure test, since opaque porcelain contains a higher
fraction of opacifiers such as zirconium or titanium oxide,
which reduce the fluidity of the slurry. The results for body
porcelain and resin composite were comparable with those determined from the four-point flexure test, since test specimens
for both materials showed a similar structure for both bi-axial
and four-point flexure test specimens. These results suggest
that this statistical approach demonstrates reasonable agreement between the bi-axial and four-point flexure strengths of
brittle specimens with similar flaw characteristics.
Comparison with diametral tensile strength.-For the diametral tensile test, it is difficult for ideal loading to be produced
along a line when cylindrical specimens are used. A proper
load distribution is generally accomplished by placement of a
narrow pad of suitable materials between the specimen and the
loading platens. For example, in the diametral tensile test procedure for ADA Specification No. 27 for direct filling resins
(Council on Dental Materials and Devices, 1977), a thin piece
of paper (approximately 0.5 mm thick) wet with water must
be inserted between the platens of the testing machine along
each side of the specimen. In ADA Specification No. 1 for
amalgam, the specimen should be padded with two thicknesses
of 0.038-mm aluminum foil on each side. However, it should
be noted that the apparent strength changes with the type of
padding material and its thickness, because the uniformity of
the tensile stress distribution also changes (Rudnick et al.,
1963). Therefore, no pad was used in the present study.
Relative to the diametral tensile test, zinc phosphate cement
exhibited a small coefficient of variation and a large Weibull
modulus, as shown in Tables 4 and 5, whereas other materials
exhibited large coefficients of variation in diametral tensile
strength and small Weibull moduli, compared with those determined from both flexure tests. Although an advantage of
the diametral tensile test is that the maximum tensile stress was
not restricted to the surface, the surface effect on the fracture
value is large (Rudnick et al., 1963). However, it is difficult
to control the surface roughness on curved surfaces. It seems

1798

BAN & ANUSA1VICE

J Dent Res December 1990

Fig. 3-SEM images of fractured surfaces that were subjected to bi-axial and four-point flexure for zinc phosphate cement (ZP), body porcelain (BP),
opaque porcelain (OP), and resin composite (RC) specimens.

Vol. 69 No. 12

FAILURE STRESS OF BRITTLE DENTAL MA TERIALS

that the surfaces of zinc phosphate cement specimens were


flattened by the initial contact of test platens, thereby yielding
a more uniform stress distribution within the specimens. Furthermore, it is well-known that the effect of specimen size on
diametral strength is large. Williams and Smith (1971) showed
that the diametral tensile strength for a zinc phosphate cement
increased with increasing diameter. Thickness-to-diameter ratios used in the present study were 0.51 + 0.01 for zinc phosphate cement, 0.46 + 0.06 for body porcelain, 0.42 0.04
for opaque porcelain, and 0.52 0.01 for resin composite.
The strength ratio of body porcelain and opaque porcelain had
a relatively large variance due to a large variance in thickness,
since these specimens were prepared by being polished. Therefore, it seems that the relatively large variance of diametral
strength for both porcelains is attributable to the inhomogeneity
of the curved surfaces and a large variance of thickness-todiameter ratio. Although resin composite had a small variance
in thickness-to-diameter ratio, it seems that the curved surface
was sufficiently inhomogeneous to decrease the variance in
strength values.
The mean diametral tensile strength of brittle dental materials was significantly lower than the bi-axial and four-point
flexure strength values, as shown in Table 4. Flexure stress
was enhanced because of the surface compression effect.
The fracture strength of brittle materials can best be explained
by postulating the presence of flaws distributed randomly
throughout the volume. Lamon (1988) showed that tensile and
bending tests provided different statistical parameters, suggesting
that different populations of flaws controlled the failure in both
cases. The flexure test specimens, in which the entire volume is
stressed fairly uniformly, should exhibit higher mean strengths
than tensile specimens (Rudnick et al., 1963). Thus, specimens
with high porosity levels, such as cement, demonstrate low diametral strength values, compared with their bi-axial flexure strength
values. For resin composite specimens, a low-degree conversion
may have occurred within the deep interior region and along the
curved surface, since light irradiation was controlled from the
flat ends of the cylindrical specimens.
It is well-recognized that the fracture strength of brittle materials depends upon several structural parameters, such as inclusions of voids and cracks (Evans, 1982), flaw location on the
surface and within the volume (Lamon and Evans, 1983), the
dimensions of specimens (Lamon and Evans, 1983), stress gradients (Ikeda et al., 1986), and the stress state (Lamon and Evans, 1983). The effects of geometry on strength can strongly
influence the results of these strength tests, and it is difficult for
the "true" tensile strength to be determined. In summary, the
bi-axial test is simpler to perform and provides a better simulation
of clinically-relevant sample size than that used for other strength
tests, since specimen size and the preparation procedures are
more similar to clinical conditions for the bi-axial test.

Acknowledgments.
The authors gratefully acknowledge Professor Jiro Hasegawa, Aichi-Gakuin University, for his helpful suggestions
and Mr. Robert B. Lee, University of Florida, for his technical
support in conducting the mechanical tests.
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